The S-bound methyl group is folded from the single N atom from the triazole ring as well as the NH band of the six-membered ring, enabling the forming of centrosymmetric eight-membered ?HNCN2 synthons in the crystal

The S-bound methyl group is folded from the single N atom from the triazole ring as well as the NH band of the six-membered ring, enabling the forming of centrosymmetric eight-membered ?HNCN2 synthons in the crystal. 0.05 mm Data collection ? Agilent SuperNova Dual diffractometer with an Atlas detector Absorption modification: multi-scan ( 2(= 0.93 2389 reflections 149 variables 1 restraint H atoms treated by an assortment of indie and constrained refinement max = 0.28 e ??3 min = ?0.29 e ??3 Data collection: (Agilent, 2011 ?); cell refinement: (Sheldrick, 2008 ?); plan(s) utilized to refine framework: (Sheldrick, 2008 ?); molecular images: (Farrugia, 2012 ?) and (Brandenburg, 2006 ?); software program used to get ready materials for publication: (Westrip, 2010 ?). ? Desk 1 Hydrogen-bond geometry (?, ) towards the thione-S2 atom. One of the most prominent feature from the crystal packaging may be the formation of centrosymmetric eight-membered HNCN2 synthons, Desk 1. They are linked into stacks along the axis by connections whereby the triazole band straddles the benzene [inter-centroid length = 3.6531 (12) ?, position of inclination = 3.04 (11)] and pyrimidine [3.7182 (12) ?, 1.90 (10)] bands of translationally related substances, Fig. 2 (symmetry procedure = 248.32= 10.5414 (11) ? = 3.1C27.5= 4.9335 (6) ? = 0.49 mm?1= 20.0943 (19) ITGA9 ?= 295 K = 99.127 (10)Prism, yellow= 1031.79 (19) ?30.30 0.15 0.05 mm= 4 Open up in another window Data collection Agilent SuperNova Dual diffractometer with an Atlas detector2389 independent reflectionsRadiation source: SuperNova (Mo) X-ray Source1667 reflections with 2(= ?1312Absorption correction: multi-scan (= ?56= ?22265096 measured reflections Open up in another window Refinement Refinement on = 0.93= 1/[2(= (and goodness of in shape derive from derive from set to no for harmful em F /em 2. The threshold appearance of em F /em 2 ( em F /em 2) can be used only for determining em R /em -elements(gt) em etc /em . and isn’t relevant to the decision of reflections for refinement. em R /em -elements predicated on em F /em 2 are statistically about doubly huge as those predicated on em F /em , and em R /em – elements predicated on ALL data will be even bigger. Open up in another home window Fractional atomic coordinates and equal or isotropic isotropic displacement variables (?2) em x /em em con /em em z /em em U /em iso*/ em U /em eqS10.57415 (5)0.09061 (12)0.69579 (3)0.03633 (18)S20.69330 (6)1.14441 (14)0.43364 (3)0.0455 (2)N10.63890 (16)0.7597 (4)0.51388 (8)0.0334 (4)H10.5735 (15)0.728 (5)0.4828 (9)0.052 (7)*N20.75333 (14)0.6491 (3)0.61961 (8)0.0288 (4)N30.74549 (16)0.4772 (3)0.67308 (8)0.0309 (4)N40.57690 (15)0.4139 (4)0.58757 (8)0.0325 (4)C10.72154 (19)0.9632 (4)0.50311 (10)0.0316 (5)C20.83231 (19)1.0021 (4)0.55680 (10)0.0306 (5)C30.92564 (19)1.1992 (5)0.55164 (11)0.0363 (5)H30.91691.31020.51380.044*C41.0296 (2)1.2317 (5)0.60125 (11)0.0403 (6)H41.09061.36400.59700.048*C51.04387 (19)1.0665 (5)0.65804 (11)0.0385 (5)H51.11511.08830.69140.046*C60.95443 (19)0.8723 (4)0.66552 (10)0.0358 (5)H60.96440.76260.70360.043*C70.84829 (18)0.8415 (4)0.61517 (10)0.0292 (5)C80.65228 (18)0.6076 (4)0.57102 (9)0.0294 (5)C90.63785 (18)0.3432 (4)0.65066 (10)0.0296 (5)C100.6908 (2)0.0885 (5)0.77103 (11)0.0474 (6)H10A0.6676?0.04560.80160.071*H10B0.69350.26370.79200.071*H10C0.77380.04610.75990.071* Open up in another home window Atomic displacement parameters (?2) em U /em 11 em U /em 22 em U /em 33 em U /em 12 em U /em 13 em U /em 23S10.0370 (3)0.0390 (4)0.0320 (3)?0.0018 (3)0.0023 (2)0.0034 (3)S20.0496 (4)0.0525 (4)0.0330 (3)?0.0007 (3)0.0019 (3)0.0110 (3)N10.0337 (9)0.0388 (11)0.0247 (9)?0.0014 (9)?0.0046 (8)0.0023 (8)N20.0291 (8)0.0321 (10)0.0237 (8)0.0019 (8)?0.0006 (7)0.0006 (8)N30.0339 (9)0.0321 (10)0.0256 (9)0.0011 (8)0.0015 (7)0.0028 (8)N40.0328 (9)0.0369 (11)0.0266 (9)0.0011 (9)0.0007 (7)0.0016 (8)C10.0351 (11)0.0320 (12)0.0285 (11)0.0054 (10)0.0070 (9)?0.0012 (9)C20.0329 (10)0.0314 (12)0.0282 (11)0.0062 (10)0.0069 (9)?0.0035 (9)C30.0380 (11)0.0367 (13)0.0354 (12)?0.0001 (11)0.0091 (10)?0.0006 (10)C40.0366 (12)0.0394 (14)0.0457 (13)?0.0061 (11)0.0090 (10)?0.0064 (12)C50.0306 (11)0.0436 (14)0.0387 (12)0.0001 (11)?0.0024 (10)?0.0089 (11)C60.0363 (11)0.0380 (13)0.0313 (11)0.0050 (10)?0.0007 (9)?0.0009 (10)C70.0287 (10)0.0304 (11)0.0283 (11)0.0020 (9)0.0044 (8)?0.0040 (9)C80.0316 (10)0.0316 (12)0.0234 (10)0.0038 (10)?0.0007 (8)?0.0027 (9)C90.0310 (10)0.0302 (12)0.0270 (10)0.0044 (10)0.0029 (9)?0.0020 (9)C100.0511 (14)0.0587 (17)0.0299 (12)?0.0044 (13)?0.0007 (10)0.0097 (12) Open up in another window Geometric variables (?, o) S1C91.738 (2)C2C31.399 (3)S1C101.791 (2)C2C71.403 (3)S2C11.645 (2)C3C41.369 (3)N1C81.360 (2)C3H30.9300N1C11.369 (3)C4C51.391 (3)N1H10.868 (10)C4H40.9300N2C81.342 (2)C5C61.369 (3)N2N31.381 (2)C5H50.9300N2C71.392 (2)C6C71.393 (3)N3C91.329 (2)C6H60.9300N4C81.319 (3)C10H10A0.9600N4C91.372 (2)C10H10B0.9600C1C21.471 (3)C10H10C0.9600C9S1C10100.05 (10)C6C5C4120.89 (19)C8N1C1123.68 (17)C6C5H5119.6C8N1H1118.3 (16)C4C5H5119.6C1N1H1118.0 (16)C5C6C7119.0 (2)C8N2N3109.51 (16)C5C6H6120.5C8N2C7123.58 (17)C7C6H6120.5N3N2C7126.91 (15)C6C7N2122.05 (19)C9N3N2101.24 (15)C6C7C2121.4 (2)C8N4C9101.80 (16)N2C7C2116.50 (17)N1C1C2115.51 (18)N4C8N2111.57 (18)N1C1S2119.93 (15)N4C8N1128.80 (17)C2C1S2124.56 (17)N2C8N1119.63 (19)C3C2C7117.51 (18)N3C9N4115.88 (18)C3C2C1121.46 (19)N3C9S1124.04 (15)C7C2C1121.0 (2)N4C9S1120.09 (15)C4C3C2121.2 (2)S1C10H10A109.5C4C3H3119.4S1C10H10B109.5C2C3H3119.4H10AC10H10B109.5C3C4C5119.9 (2)S1C10H10C109.5C3C4H4120.0H10AC10H10C109.5C5C4H4120.0H10BC10H10C109.5C8N2N3C90.5 (2)C3C2C7C6?1.4 (3)C7N2N3C9179.49 (18)C1C2C7C6178.41 (19)C8N1C1C22.8 (3)C3C2C7N2179.17 (17)C8N1C1S2?177.27 (16)C1C2C7N2?1.0 (3)N1C1C2C3178.67 (19)C9N4C8N21.2 (2)S2C1C2C3?1.3 (3)C9N4C8N1?178.6 (2)N1C1C2C7?1.2 (3)N3N2C8N4?1.2 (2)S2C1C2C7178.89 (16)C7N2C8N4179.82 (17)C7C2C3C40.9 (3)N3N2C8N1178.65 (17)C1C2C3C4?178.9 (2)C7N2C8N1?0.4 (3)C2C3C4C50.1 (3)C1N1C8N4177.7 (2)C3C4C5C6?0.6 (3)C1N1C8N2?2.1 (3)C4C5C6C70.1 (3)N2N3C9N40.3 (2)C5C6C7N2?179.68 (19)N2N3C9S1179.79 (14)C5C6C7C21.0 (3)C8N4C9N3?0.9 (2)C8N2C7C6?177.57 (19)C8N4C9S1179.53 (15)N3N2C7C63.6 (3)C10S1C9N30.4 (2)C8N2C7C21.8 (3)C10S1C9N4179.93 (17)N3N2C7C2?177.02 (18) Open up in another home window Hydrogen-bond.deviation from the non-H atoms = 0.041??). & Geffken (2010 ?, 2011 ?); Al-Salahi (2011 ?, 2013 ?). Experimental ? Crystal data ? C10H8N4S2 = 248.32 Monoclinic, = 10.5414 (11) ? = 4.9335 (6) ? = 20.0943 (19) ? = 99.127 (10) = 1031.79 (19) ?3 = 4 Mo = 295 K 0.30 Ixazomib citrate 0.15 0.05 mm Data collection ? Agilent SuperNova Dual diffractometer with an Atlas detector Absorption modification: multi-scan ( 2(= 0.93 2389 reflections 149 variables 1 restraint H atoms treated by an assortment of indie and constrained refinement max = 0.28 e ??3 min = ?0.29 e ??3 Data collection: (Agilent, 2011 ?); cell refinement: (Sheldrick, 2008 ?); plan(s) utilized to refine framework: (Sheldrick, 2008 ?); molecular images: (Farrugia, 2012 ?) and (Brandenburg, 2006 ?); software program used to get ready materials for publication: (Westrip, 2010 ?). ? Desk 1 Hydrogen-bond geometry (?, ) towards the thione-S2 atom. One of the most prominent feature from the crystal packaging may be the formation of centrosymmetric eight-membered HNCN2 synthons, Desk 1. They are linked into stacks along the axis by connections whereby the triazole band straddles the benzene [inter-centroid length = 3.6531 (12) ?, position of Ixazomib citrate inclination = 3.04 (11)] and pyrimidine [3.7182 (12) ?, 1.90 (10)] bands of translationally related substances, Fig. 2 (symmetry procedure = 248.32= 10.5414 (11) ? = 3.1C27.5= 4.9335 (6) ? = 0.49 mm?1= 20.0943 (19) ?= 295 K = 99.127 (10)Prism, yellow= 1031.79 (19) ?30.30 0.15 0.05 mm= 4 Open up in another window Data collection Agilent SuperNova Dual diffractometer with an Atlas detector2389 independent reflectionsRadiation source: SuperNova (Mo) X-ray Source1667 reflections with 2(= ?1312Absorption correction: multi-scan (= ?56= ?22265096 measured reflections Open up in another window Refinement Refinement on = 0.93= 1/[2(= (and goodness of in shape derive from derive from set to no for harmful em F /em 2. The threshold appearance of em F /em 2 ( em F /em 2) can be used only for determining em R /em -elements(gt) em etc /em . and isn’t relevant to the decision of reflections for refinement. em R /em -elements predicated on em F /em 2 are statistically about doubly huge as those predicated on em F /em , and em R /em – elements predicated on ALL data will end up being even bigger. Open in another home window Fractional atomic coordinates and isotropic or comparable isotropic displacement variables (?2) em x /em em con /em em z /em em U /em iso*/ em U /em eqS10.57415 (5)0.09061 (12)0.69579 (3)0.03633 (18)S20.69330 (6)1.14441 (14)0.43364 (3)0.0455 (2)N10.63890 (16)0.7597 (4)0.51388 (8)0.0334 (4)H10.5735 (15)0.728 (5)0.4828 (9)0.052 (7)*N20.75333 (14)0.6491 (3)0.61961 (8)0.0288 (4)N30.74549 (16)0.4772 (3)0.67308 (8)0.0309 (4)N40.57690 (15)0.4139 (4)0.58757 (8)0.0325 (4)C10.72154 (19)0.9632 (4)0.50311 (10)0.0316 (5)C20.83231 (19)1.0021 (4)0.55680 (10)0.0306 (5)C30.92564 (19)1.1992 (5)0.55164 (11)0.0363 (5)H30.91691.31020.51380.044*C41.0296 (2)1.2317 (5)0.60125 (11)0.0403 (6)H41.09061.36400.59700.048*C51.04387 (19)1.0665 (5)0.65804 (11)0.0385 (5)H51.11511.08830.69140.046*C60.95443 (19)0.8723 (4)0.66552 (10)0.0358 (5)H60.96440.76260.70360.043*C70.84829 (18)0.8415 (4)0.61517 (10)0.0292 (5)C80.65228 (18)0.6076 (4)0.57102 (9)0.0294 Ixazomib citrate (5)C90.63785 (18)0.3432 (4)0.65066 (10)0.0296 (5)C100.6908 (2)0.0885 (5)0.77103 (11)0.0474 (6)H10A0.6676?0.04560.80160.071*H10B0.69350.26370.79200.071*H10C0.77380.04610.75990.071* Open up in another home window Atomic displacement parameters (?2) em U /em 11 em U /em 22 em U /em 33 em U /em 12 em U /em 13 em U /em 23S10.0370 (3)0.0390 (4)0.0320 (3)?0.0018 (3)0.0023 (2)0.0034 (3)S20.0496 (4)0.0525 (4)0.0330 (3)?0.0007 (3)0.0019 (3)0.0110 (3)N10.0337 (9)0.0388 (11)0.0247 (9)?0.0014 (9)?0.0046 (8)0.0023 (8)N20.0291 (8)0.0321 (10)0.0237 (8)0.0019 (8)?0.0006 (7)0.0006 (8)N30.0339 (9)0.0321 (10)0.0256 (9)0.0011 (8)0.0015 (7)0.0028 (8)N40.0328 (9)0.0369 (11)0.0266 (9)0.0011 (9)0.0007 (7)0.0016 (8)C10.0351 (11)0.0320 (12)0.0285 (11)0.0054 (10)0.0070 (9)?0.0012 (9)C20.0329 (10)0.0314 (12)0.0282 (11)0.0062 (10)0.0069 (9)?0.0035 (9)C30.0380 (11)0.0367 (13)0.0354 (12)?0.0001 (11)0.0091 (10)?0.0006 (10)C40.0366 (12)0.0394 (14)0.0457 (13)?0.0061 (11)0.0090 (10)?0.0064 (12)C50.0306 (11)0.0436 (14)0.0387 (12)0.0001 (11)?0.0024 (10)?0.0089 (11)C60.0363 (11)0.0380 (13)0.0313 (11)0.0050 (10)?0.0007 (9)?0.0009 (10)C70.0287 (10)0.0304 (11)0.0283 (11)0.0020 (9)0.0044 (8)?0.0040 (9)C80.0316 (10)0.0316 (12)0.0234 (10)0.0038 (10)?0.0007 (8)?0.0027 (9)C90.0310 (10)0.0302 (12)0.0270 (10)0.0044 (10)0.0029 (9)?0.0020 (9)C100.0511 (14)0.0587 (17)0.0299 (12)?0.0044 (13)?0.0007 (10)0.0097 (12) Open up in another window Geometric variables (?, o) S1C91.738 (2)C2C31.399 (3)S1C101.791 (2)C2C71.403 (3)S2C11.645 (2)C3C41.369 (3)N1C81.360 (2)C3H30.9300N1C11.369 (3)C4C51.391 (3)N1H10.868 (10)C4H40.9300N2C81.342 (2)C5C61.369 (3)N2N31.381 (2)C5H50.9300N2C71.392 (2)C6C71.393 (3)N3C91.329 (2)C6H60.9300N4C81.319 (3)C10H10A0.9600N4C91.372 (2)C10H10B0.9600C1C21.471 (3)C10H10C0.9600C9S1C10100.05 (10)C6C5C4120.89 (19)C8N1C1123.68 (17)C6C5H5119.6C8N1H1118.3 (16)C4C5H5119.6C1N1H1118.0 (16)C5C6C7119.0 (2)C8N2N3109.51 (16)C5C6H6120.5C8N2C7123.58 (17)C7C6H6120.5N3N2C7126.91 (15)C6C7N2122.05 (19)C9N3N2101.24 (15)C6C7C2121.4 (2)C8N4C9101.80 (16)N2C7C2116.50 (17)N1C1C2115.51 (18)N4C8N2111.57 (18)N1C1S2119.93 (15)N4C8N1128.80 (17)C2C1S2124.56 (17)N2C8N1119.63 (19)C3C2C7117.51 (18)N3C9N4115.88 (18)C3C2C1121.46 (19)N3C9S1124.04 (15)C7C2C1121.0 (2)N4C9S1120.09 (15)C4C3C2121.2 (2)S1C10H10A109.5C4C3H3119.4S1C10H10B109.5C2C3H3119.4H10AC10H10B109.5C3C4C5119.9 (2)S1C10H10C109.5C3C4H4120.0H10AC10H10C109.5C5C4H4120.0H10BC10H10C109.5C8N2N3C90.5 (2)C3C2C7C6?1.4 (3)C7N2N3C9179.49 (18)C1C2C7C6178.41 (19)C8N1C1C22.8 (3)C3C2C7N2179.17 (17)C8N1C1S2?177.27 (16)C1C2C7N2?1.0 (3)N1C1C2C3178.67 (19)C9N4C8N21.2 (2)S2C1C2C3?1.3 (3)C9N4C8N1?178.6 (2)N1C1C2C7?1.2 (3)N3N2C8N4?1.2 (2)S2C1C2C7178.89 (16)C7N2C8N4179.82 (17)C7C2C3C40.9 (3)N3N2C8N1178.65 (17)C1C2C3C4?178.9 (2)C7N2C8N1?0.4 (3)C2C3C4C50.1 (3)C1N1C8N4177.7 (2)C3C4C5C6?0.6 (3)C1N1C8N2?2.1 (3)C4C5C6C70.1 (3)N2N3C9N40.3 (2)C5C6C7N2?179.68 (19)N2N3C9S1179.79 (14)C5C6C7C21.0 (3)C8N4C9N3?0.9 (2)C8N2C7C6?177.57 (19)C8N4C9S1179.53 (15)N3N2C7C63.6 (3)C10S1C9N30.4 (2)C8N2C7C21.8 (3)C10S1C9N4179.93 (17)N3N2C7C2?177.02 (18) Open up in another home window Hydrogen-bond geometry (?, o) em D /em H em A /em em D /em HH em A /em em D /em em A /em em D /em H em A /em N1H1N4we0.87 (1)2.07 (1)2.931 (2)171 (2) Open up in another home window Symmetry code: (i) ? em x /em +1, ? em /em +1 y, ? em z /em +1. Footnotes Supplementary data and statistics because of this paper can be found through the IUCr digital archives (Guide: HB7045)..

Related Posts

Begin typing your search term above and press enter to search. Press ESC to cancel.

Back To Top